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Chapmanite [Fe2sb(Si2o5)O3(OH)]: Thermodynamic Properties and Formation in Low-Temperature Environments

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Chapmanite [Fe2sb(Si2o5)O3(OH)]: Thermodynamic Properties and Formation in Low-Temperature Environments Eur. J. Mineral., 33, 357–371, 2021 https://doi.org/10.5194/ejm-33-357-2021 © Author(s) 2021. This work is distributed under the Creative Commons Attribution 4.0 License. Chapmanite [Fe2Sb(Si2O5)O3(OH)]: thermodynamic properties and formation in low-temperature environments Juraj Majzlan1, Stefan Kiefer1, Kristina Lilova2, Tamilarasan Subramani2, Alexandra Navrotsky2, Edgar Dachs3, and Artur Benisek3 1Institute of Geosciences, Friedrich Schiller University, Burgweg 11, 07749 Jena, Germany 2School of Molecular Sciences and Center for Materials of the Universe, Arizona State University, Tempe, Arizona 85287, USA 3Department of Chemistry and Physics of Materials, University of Salzburg, Jakob-Haringer-Str. 2a, 5020 Salzburg, Austria Correspondence: Juraj Majzlan ([email protected]) Received: 18 March 2021 – Revised: 1 June 2021 – Accepted: 4 June 2021 – Published: 2 July 2021 Abstract. In this work, we have determined or evaluated thermodynamic properties of synthetic Sb2O5, MgSb2O6 (analogue of the mineral byströmite), Mg[Sb(OH)6]2 · 6H2O (brandholzite), and natural chapman- ite [(Fe1:88Al0:12)Sb(Si2O5)O3(OH)]. Enthalpies of reactions, including formation enthalpies, were evaluated using reference compounds Sb, Sb2O3, Sb2O5, and other phases, with high-temperature oxide melt solution calorimetry in lead borate and sodium molybdate solvents. Heat capacity and entropy were determined by relax- o −1 o −1 −1 ation and differential scanning calorimetry. The best set of 1f H (kJ mol ) and S (J mol K ) is byströmite −1733:0±3:6, 139:3±1:0; brandholzite −5243:1±3:6, 571:0±4:0; and chapmanite −3164:9±4:7, 305:1±2:1. o −1 The data for chapmanite give 1f G of −2973:6 ± 4:7 kJ mol and logK D −17:10 for the dissolution reac- C C ! 3C C 3C C 0 C 0 C tion (Fe1:88Al0:12)Sb(Si2O5)O3(OH) 6H 1.88Fe 0.12Al 2SiO2 Sb(OH)3 2H2O. Analysis of the data showed that chapmanite is finely balanced in terms of its stability with schafarzikite (FeSb2O4) and tripuhyite (FeSbO4) under a specific, narrow range of conditions when both aqueous Fe(III) and Sb(III) are abun- 0 dant. In such a model, chapmanite is metastable by a narrow margin but could be stabilized by high SiO2(aq) activities. Natural assemblages of chapmanite commonly contain abundant amorphous silica, suggesting that this mechanism may be indeed responsible for the formation of chapmanite. Chapmanite probably forms dur- ing low-temperature hydrothermal overprint of pre-existing Sb ores under moderately reducing conditions; the slightly elevated temperatures may help to overcome the kinetic barrier for its crystallization. During weathering, sheet silicates may adsorb Sb3C in tridentate hexanuclear fashion, thus exposing their chapmanite-like surfaces to the surrounding aqueous environment. Formation of chapmanite, as many other sheet silicates, under ambient conditions, is unlikely. 1 Introduction zlan et al.(2016). The rich mineralogy of antimony was ex- tensively summarized by Majzlan(2021), and the details will Antimony is an element that enters into both quite soluble not be repeated here. and quite insoluble minerals as it moves through the aque- Two insoluble minerals, considered to be the “ultimate 5C ous environment. The solubility of such reservoirs was pre- sinks” of antimony, are tripuhyite (FeSb O4) and scha- viously quantified by Filella and May(2003), Diemar et al. 3C farzikite (FeSb2 O4)(Leverett et al., 2012). Tripuhyite has (2009), Leverett et al.(2012), Roper et al.(2015), and oth- been identified at a number of sites polluted by Sb (see Ma- ers using thermodynamic data. The discrepancies between jzlan, 2021), but schafarzikite is rare, restricted to a few lo- the observations of antimony being soluble at some sites but calities where it seems to be primary and not secondary (e.g., insoluble at other ones were addressed and resolved by Maj- Published by Copernicus Publications on behalf of the European mineralogical societies DMG, SEM, SIMP & SFMC. 358 J. Majzlan et al.: Thermodynamics of chapmanite Table 1. Chemical formulae and mineral names of phases investi- 2 Materials gated in this work. With the exception of chapmanite, all samples used in this work were synthetic. Space groups and refined lattice Synthetic Sb2O3 (equivalent of valentinite) and Sb2O5 were parameters for the antimony phases can be found in Table 2. purchased from suppliers and used as received. Sb2O4 (equivalent of cervantite) was synthesized by treatment of ◦ Sb2O3 valentinite Sb2O3 at 700 C for 1 d (Konopik and Zwiauer, 1952). Pow- Sb2O4 cervantite dery Sb2O3 was placed into a platinum crucible, covered by Sb2O5 · nH2O– a platinum lid and heated in air. In contrast to the results of · Mg[Sb(OH)6]2 6H2O brandholzite Konopik and Zwiauer(1952), we found that prolonged heat MgSb2O6 byströmite treatment does not lead to better crystallinity or phase purity Fe Sb(Si O )O (OH) chapmanite 2 2 5 3 but to amorphization of the sample. Fe O hematite 2 3 · MgO periclase Crystals of Mg[Sb(OH)6]2 6H2O (equivalent of brand- holzite) were synthesized according to the procedure of SiO2 quartz Diemar et al.(2009). Two separate solutions were prepared initially. One of them was 1 M Sb5C solution, prepared by mixing deionized water and KSb(OH) . The suspension was Sejkora et al., 2007). Its rarity could be explained by the 6 heated on a heating plate at ≈ 60 ◦C until most of the solid scarcity of research in reduced environments because most dissolved. The undissolved residue was separated by de- of the work at the polluted sites is concentrating on their ox- cantation. The other solution was 0.1 M Mg2C, prepared by idized portions. They are believed to release toxic elements, mixing of deionized water and MgCl · 6H O. The two so- such as antimony, into the environment. An alternative expla- 2 2 lutions were mixed, resulting in the immediate formation of nation is that schafarzikite does not form since its nucleation a white precipitate. The suspension was allowed to stand at and growth is kinetically hindered. Another possibility is that room temperature for 2 months and then filtered and washed there is a competing phase or phases that scavenge antimony several times by deionized water. The filtrate consisted of eu- under such conditions. Iron oxides, the usual scavengers of hedral crystals of Mg[Sb(OH) ] ·6H O and white, powdery many anions, are not good candidates, as they may undergo 6 2 2 aggregates of an unknown phase, perhaps of the same com- reductive dissolution under such conditions. On the other position. The crystals were up to 1 mm in size and were sep- hand, it has been shown that during reduction–oxidation cy- arated from the rest of the sample under a binocular micro- cles antimony adsorbed onto goethite will be locked into scope. tripuhyite and not into the structure of schafarzikite (Burton MgSb O was prepared from Mg[Sb(OH) ] · 6H O by et al., 2020). 2 6 6 2 2 heating at 1000 ◦C for 1 h. The crystals of Mg(Sb(OH) ) · The aim of this work is to evaluate the thermodynamic 6 2 6H O were placed into a platinum crucible, covered by a stability of chapmanite, a rare mineral that could, however, 2 platinum lid and heated in air. The resulting sample was pow- constitute an alternative sink of antimony in slightly reduc- dery and grayish. ing environments. To this goal, first we verified the method- A natural sample of chapmanite, nominally ology of high-temperature oxide melt solution calorimetry in Fe Sb(Si O )O (OH), used in this work originated from the molten lead borate on antimony phases, doing a number of 2 2 5 3 Pezinok Sb deposit in Slovakia (Polák, 1983, 1988). The cross-checks. Once assured that this method can yield accu- sample consisted of a coating of powdery greenish-yellow rate and precise data, the enthalpy of formation of chapman- crusts of chapmanite on dark gray quartz with sparse tiny ite was measured. Entropy was obtained by integration of pyrite crystals. The crusts were scraped of the specimens low-temperature heat capacity data measured by relaxation and separated by a standard protocol for clay mineral calorimetry. Calculations of stability and solubility of chap- separation. Briefly, 20 g of the sample under 0.16 mm (after manite in selected exemplary systems document its possible grinding) was mixed with 300 mL distilled water in a beaker. role in the environment. Afterwards, 3–4 mL of 0.1 M solution of sodium hexam- Throughout this paper, the phases investigated can be re- etaphosphate were added, the suspension was ultrasonicated ferred to by their mineral names. In their synthetic form, they for 5 min, the volume added up to 2 L in a cylinder. After are equivalents of the naturally occurring minerals. The use 24 h, the water column was removed with a suction pump of these names improves the clarity of the presentation be- and the sediment at the bottom discarded. The suspension cause a mineral name is linked not only to a specific chemical from the suction pump was transferred into a beaker, and composition, but also to a crystal structure. It is particularly a few drops of 15 % HCl were added to coagulate the clay advantageous in systems with polymorphism, such as among particles. After coagulation, water was removed with the the antimony oxides. The chemical formulae and mineral suction pump and discarded. The slurry was transferred onto names of the phases considered in this paper are summarized a thin plastic sheet and dried at 50 ◦C. Further treatment, in Table 1. owing to the analytical results, is described below. Eur. J. Mineral., 33, 357–371, 2021 https://doi.org/10.5194/ejm-33-357-2021 J.
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